CN111979578B - Heat radiation reflection device for producing silicon carbide single crystal and preparation method and application thereof - Google Patents
Heat radiation reflection device for producing silicon carbide single crystal and preparation method and application thereof Download PDFInfo
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- CN111979578B CN111979578B CN202010663166.7A CN202010663166A CN111979578B CN 111979578 B CN111979578 B CN 111979578B CN 202010663166 A CN202010663166 A CN 202010663166A CN 111979578 B CN111979578 B CN 111979578B
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/38—Borides
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
Abstract
The application discloses a heat radiation reflecting device for producing silicon carbide single crystals and a preparation method and application thereof. The device can form a thermal radiation reflecting mirror surface, the thermal radiation reflecting mirror surface can surround the periphery of a crystal growth crucible for producing silicon carbide single crystals by a PVT method, and the heat emitted from the crucible can be reflected back to the crucible. Experiments prove that the device arranged on the periphery of the PVT method silicon carbide crystal growth crucible can reduce the power for crystal growth, save electric energy and crystal growth cost, reduce the defects of crystal polytype, microtubule and the like of the silicon carbide crystal and improve the yield; in addition, the heat is mainly reflected to the crucible after the device is used, the heat conducted outwards is little, the outside of the device for producing the silicon carbide single crystal by the PVT method does not need to be cooled, the cooling mode of circulating water or air inlets and air outlets outside the crystal growth device is replaced, and the fluctuation probability of crystal growth conditions is reduced.
Description
Technical Field
The invention relates to the field of silicon carbide single crystal production processes, in particular to a heat radiation reflecting device for producing silicon carbide single crystals by a PVT method and a preparation method and application thereof.
Background
Silicon carbide is one of the third generation wide bandgap semiconductor materials following silicon and gallium arsenide, and is widely applied to the fields of power electronics, radio frequency devices, photoelectronic devices and the like because of its excellent properties such as large forbidden bandwidth, high saturated electron mobility, strong breakdown field, high thermal conductivity and the like. High quality crystals are the cornerstone of semiconductor and information industry development, and the level of their fabrication limits the fabrication and performance of downstream devices. Although Physical Vapor Transport (PVT) growth of silicon carbide crystals has advanced sufficiently in recent years, the stability of the grown crystals needs to be further studied, for example, the crystal growth process is influenced by the fluctuation of the temperature of circulating water, and the power consumption of the silicon carbide crystal growth process is too large.
At present, the cooling mode outside the furnace chamber of the crystal growing furnace for growing the silicon carbide crystal mainly comprises two modes: the two methods are limited by the control of the temperature of circulating water, if the temperature of the circulating water fluctuates, the crystal growth condition fluctuates, the final result causes the fluctuation of the crystal growth condition to influence the crystal growth stability, the defects of polytype, microtubule and the like of the crystal are caused, and the yield is influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a heat radiation reflecting device for producing silicon carbide single crystals and a preparation method and application thereof.
In one aspect, the present invention provides a heat radiation reflecting apparatus for producing a silicon carbide single crystal by a PVT process, the apparatus being capable of forming a heat radiation reflecting mirror surface capable of surrounding a periphery (e.g., a side periphery and/or an upper portion and/or a lower portion) of a growth crucible for producing a silicon carbide single crystal by a PVT process, and capable of reflecting heat emitted from the crucible (including an inside and/or an outside of the crucible) back to the crucible (including an inside and/or an outside of the crucible).
In the above-described heat radiation reflecting device, the vacuum shielding case may be covered outside the crucible, and the specific material layer may be provided on an inner surface of the vacuum shielding case, and preferably, the inner surface of the vacuum shielding case is made of quartz; or
The heat radiation reflecting device comprises a support and a specific material layer arranged on one side of the support;
when the silicon carbide single crystal is produced by the PVT method, the support/the vacuum isolation cover and the specific material layer surround the periphery of a crystal growth crucible for producing the silicon carbide single crystal by the PVT method, and the melting point of the support/the vacuum isolation cover and the melting point of the specific material are higher than the highest temperature at the positions of the support/the vacuum isolation cover and the specific material; the highest temperature refers to the corresponding temperature when the silicon carbide single crystal is produced by a PVT method;
the material of the support/the vacuum isolation cover can be the same as the specific material (for example, the material of the support is a metal, one side of the support can be used as a heat radiation reflection mirror), or can be different (for example, a metal coating is arranged on the surface of quartz glass);
wherein the thermal radiation reflecting mirror surface is an outer surface of the specific material layer, and/or,
the heat radiation reflecting mirror surface is an interface between the support and the specific material layer, and the support is made of a transparent material, preferably, quartz glass.
In the above-described heat radiation reflecting device, the specific material is a metal, a silicon compound, a boride, a carbide or a nitride, more preferably, a metal;
the metal includes: tantalum, tungsten, molybdenum, iridium, niobium, germanium, hafnium, or alloys thereof, more preferably, tantalum;
the boride comprises: boron carbide, boron nitride, zirconium boride, lanthanum boride, titanium boride, tantalum boride, chromium boride, tungsten boride, molybdenum boride, vanadium boride, or niobium boride;
the carbide includes: chromium carbide, tantalum carbide, vanadium carbide, zirconium carbide, tungsten carbide, molybdenum carbide, titanium carbide, or niobium carbide, preferably, tantalum carbide;
the nitride includes: titanium nitride, tungsten nitride, molybdenum nitride, chromium nitride, niobium nitride, zirconium nitride, tantalum nitride, or vanadium nitride.
In the above-described heat radiation reflecting device, the specific material is a metal, the metal is tantalum, and the thickness of the specific material layer is 3 μm or more, or 4 to 100 μm, more preferably 5 to 60 μm, more preferably 10 to 40 μm, more preferably 15 to 35 μm;
and/or the roughness of the heat radiation reflecting mirror surface is less than 25 μm, preferably the roughness of the heat radiation reflecting mirror surface is less than 15 μm.
The thickness of the specific material layer can be determined according to actual conditions and requirements such as different components of the specific material, different distances between the specific material layer and the outer wall of the crucible, energy consumption requirements and the like;
the smaller the thickness of the specific material layer is, the weaker the heat reflection effect is, and the lower the cost is;
the greater the thickness of the specific material layer, the stronger the effect of reflecting heat, but the higher the cost;
the larger the distance between the specific material layer and the crucible is, the weaker the effect of reflecting heat is, and the stronger the effect is otherwise;
the test results of the embodiment of the application show that when the thickness of Ta is less than 5 μm, the Ta is not compact enough, the crystal quality can only be improved but the energy consumption can not be obviously reduced, but when the thickness of Ta is 15-35 μm or more, the Ta can not only improve the crystal quality but also obviously reduce the energy consumption.
In practice, the melting point of the specific material may be greater than or equal to the melting point of the material of the inner surface of the support/the vacuum isolation cover, and the specific material is inactive and does not introduce impurities into the silicon carbide single crystal.
Generally, the device for producing silicon carbide single crystal by the PVT method, such as a crystal growth furnace, is a vacuum cavity body made of a quartz tube, and the temperature which the specific material needs to bear is at least equal to or higher than the melting point (1750 ℃) of the quartz tube, so that the safe production can be ensured.
The method for plating the specific material layer on the inner surface or the outer surface of the vacuum isolation cover is not limited to the vacuum plating method such as PVD (physical vapor deposition), CVD (chemical vapor deposition) and the like,
the PVD comprises vacuum evaporation, sputtering coating, arc plasma coating, ion coating and molecular beam epitaxy; the CVD comprises atmospheric pressure chemical vapor deposition, low pressure chemical vapor deposition and plasma chemical vapor deposition which has the characteristics of both CVD and PVD;
the embodiment of the application is specifically sputtering coating.
In another aspect, the present invention provides a method for producing the heat radiation reflecting device as defined in any of the above, the method comprising coating an inner surface of the vacuum insulation cover or an inner surface or an outer surface of the support with a vacuum coating method to obtain the heat radiation reflecting device in which the specific material layer and the heat radiation reflecting mirror surface are formed on the inner surface of the vacuum insulation cover or the inner surface or the outer surface of the support.
In the above preparation method, the vacuum coating method is PVD or CVD; preferably, the PVD is a sputter coating. High-purity target materials are used for coating, and the denser the coating, the fewer defects (such as point defects or line defects) in the film are, the better the film is.
In the above preparation method, the sputter coating method comprises the steps of:
1) cleaning the vacuum isolation cover or the support as a substrate by using acetone and then deionized water;
2) background vacuum degree of shooting chamber is 1.0 x 10-4～9.9×10-4Pa or 1.0X 10-5～9.9×10-5Pa, introducing argon with the purity not lower than 99.99% into a coating chamber for 0.5-1 h before sputtering, and keeping the pressure at 0.1-1.5 Pa;
3) and (2) performing target sputtering on the substrate by using the metal with the purity of not less than 99.999% as a target material, wherein the sputtering power is 40-60W, the sputtering gas is argon with the purity of not less than 99.99%, the gas pressure is 0.2-2.7 Pa, and the sputtering is performed for 2-3h to obtain the heat radiation reflecting device with the specific material being metal (such as tantalum).
When the coating film is formed, namely the specific material layer is coated on the outer surface of the vacuum isolation cover, the specific material is easily oxidized by high temperature during actual production, so that the effect of a thermal radiation reflecting mirror surface is lost, and finally the thermal radiation reflecting device cannot play a good heat preservation effect.
Optionally, the substrate has a surface roughness of no greater than 10 μm. Preferably, the surface roughness of the substrate is in the range of 5-10 μm. The setting mode of the surface roughness of the substrate enables the surface of the coating layer contacted with the substrate to be compact and the coating layer effect to be good.
In another aspect, the present invention provides the use of any one of the above-described thermal radiation reflecting devices, or the thermal radiation reflecting device obtained by the above-described method, in the production of a silicon carbide single crystal by the PVT method,
preferably, the application is to improve the quality of the silicon carbide single crystal produced by the PVT method and/or reduce the energy consumption of the silicon carbide single crystal produced by the PVT method;
more preferably, the improving the quality of the silicon carbide single crystal produced by the PVT method comprises the following steps: the crystal polytype (e.g., area), lattice distortion, number of micropipes, and/or micropipe density in a silicon carbide single crystal are reduced.
The invention has the following beneficial effects:
experiments prove that the thermal radiation reflecting device arranged on the periphery of the PVT method silicon carbide crystal growth crucible can reflect heat radiated from the interior of the crystal growth crucible back to the interior of the crucible, so that the power for crystal growth is reduced, the electric energy and the crystal growth cost are saved, the defects of crystal polytype, micropipe and the like of the silicon carbide crystal can be reduced, and the yield is improved; in addition, the heat is mainly reflected to the crucible after the heat radiation reflection device is used, the heat conducted outwards is little, the outside of the device for producing the silicon carbide single crystal by the PVT method does not need to be cooled, the cooling mode of circulating water or air inlets and air outlets outside the crystal growth device is replaced, and the fluctuation probability of crystal growth conditions is reduced.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a longitudinal sectional view of a heat radiation reflecting apparatus for producing a silicon carbide single crystal by the PVT method.
FIG. 2 is a longitudinal sectional view of another heat radiation reflecting apparatus for producing a silicon carbide single crystal by the PVT method.
Fig. 3 is a longitudinal sectional view of the apparatus of fig. 1 in an apparatus or production of a silicon carbide single crystal by the PVT method.
Fig. 4 is an enlarged view and a schematic diagram of a portion of the structure of fig. 3 in a dashed line.
FIG. 5 shows the results of half height width measurement of XRD of a silicon carbide single crystal sample.
The reference numerals in the figures are as follows:
1 crucible, 2 temperature monitoring devices, 3-1 vacuum isolation hood (specifically quartz tube), 3-2 support, 4 heat preservation structures, 5 heating devices, 6 metal coating, 7 seed crystals, 8 raw materials and 9 vacuum systems.
Detailed Description
EXAMPLE 1 Heat radiation reflecting apparatus for producing silicon carbide Single Crystal
As shown in FIG. 1, the heat radiation reflecting device for producing a silicon carbide single crystal according to the present embodiment comprises a single-layered vacuum insulation cover 3-1 and a metal plating layer 6 plated on the inner surface of the vacuum insulation cover 3-1;
the vacuum isolation cover 3-1 can cover the periphery of the crystal growth crucible 1 for producing the silicon carbide single crystal by the PVT method;
the outer surface (specifically, the side outer surface, and may also include the upper outer surface) of the metal plating layer 6 can form a heat radiation reflection mirror surface;
the metal coating 6 is made of tantalum (Ta); the thickness of the metal plating layer 6 is 3 μm or more, preferably, 4 to 100 μm, more preferably, 5 to 60 μm, more preferably, 10 to 40 μm, more preferably, 15 to 35 μm;
the vacuum insulation hood 3-1 has the same shape as the crucible 1 inside when in use, and is cylindrical so that the two are coaxial and the outside and/or inside of the crucible 1 is uniformly heated.
The preparation method (PVD-sputtering coating) of the metal coating 6 is as follows:
background vacuum degree of shooting chamber is 1.0 x 10-4～9.9×10-4Pa or 1.0X 10-5～9.9×10-5Pa, introducing 99.99 percent purity argon into the film coating chamber for 0.5 to 1 hour before sputtering, and maintaining the pressure at 0.1 to 1.5 Pa; during sputtering, the pressure of high-purity argon with the purity of 99.99% is 0.2-2.7 Pa, a vacuum isolation cover 3-1 (namely a quartz tube) is firstly cleaned by acetone and then by deionized water, sputtering is carried out by adopting a high-purity Ta target with the purity of 99.999% for 2-3 hours at the sputtering power of 50W, and a metal coating 6 is obtained, and the thickness of the metal coating is measured by a step instrument method or an XRT method.
As a result: the compact surface of the plating layer is a smooth mirror surface, and the roughness of the mirror surface is less than 25 mu m.
EXAMPLE 2 Heat radiation reflecting apparatus for producing silicon carbide Single Crystal
The difference from the embodiment 1 is that: the metal plating layer 6 is plated on the outer surface of the support 3-2 (fig. 2), the interface of the support 3-2 and the metal plating layer 6 forms a heat radiation reflection mirror surface,
the support 3-2 is made of quartz glass, the shape of the support is the same as that of the crucible 1 in the inner part when in use, in particular to be cylindrical, so that the support and the crucible are coaxial, the outer part and/or the inner part of the crucible 1 are heated uniformly, the support 3-2 only has the function of supporting the metal coating 6 and does not have the function of vacuum isolation,
in the production of silicon carbide single crystal by the PVT method, the heat radiation reflecting device of the present embodiment should be placed outside the crucible 1 and inside the vacuum insulation cover 3-1.
EXAMPLE 3 Heat radiation reflecting apparatus for producing silicon carbide Single Crystal
The difference from the embodiment 1 is that: the material of the metal plating layer 6 is TaC.
EXAMPLE 4 Heat radiation reflecting apparatus for producing silicon carbide Single Crystal
The difference from the embodiment 2 is that: the material of the metal plating layer 6 is TaC.
Other embodiments of the above-described heat radiation reflecting apparatus for producing a silicon carbide single crystal are as follows:
1) in another embodiment, the vacuum isolation cover 3-1 can also be a double layer, and the middle part of the double layer is a vacuum layer;
2) in another embodiment, the vacuum insulation cover 3-1/the support 3-2 has a spherical shape, and the crucible 1 inside thereof has a spherical shape, and they are concentric to each other, so that the crucible 1 is uniformly heated from the outside and/or the inside thereof.
The use method of the heat radiation reflecting device for producing a silicon carbide single crystal by taking fig. 3 as an example is as follows:
as shown in FIG. 3, any of the above-mentioned heat radiation reflecting devices is placed on the outer periphery of a crucible 1 in an apparatus for producing a silicon carbide single crystal by the PVT method, and a heat radiation reflecting mirror surface can reflect heat emitted from the crucible 1 back to the crucible 1 (FIG. 4),
wherein, the device for producing the silicon carbide single crystal by the PVT method comprises: the device comprises a silicon carbide crystal growth crucible 1, a temperature monitoring device 2, a heat preservation structure 4, a heating device 5 and a vacuum system 9;
the temperature monitoring device 2 can monitor the internal temperature of the crucible 1 (graphite crucible), and comprises a pyrometer arranged above the crucible 1;
the vacuum system 9 is arranged above the vacuum isolation cover 3-1, can vacuumize a growth cavity in the crystal growth crucible 1 and detect the vacuum degree, and specifically comprises a mechanical pump, a molecular pump and a vacuum degree measuring device;
the heat insulation structure 4 is positioned outside the crucible 1 and in the heat radiation reflection device;
the heating device 5 is specifically a heating coil, and can heat the crucible 1;
the device for producing the silicon carbide single crystal by the PVT method does not comprise a cooling device or comprises the cooling device, but the cooling function of the cooling device is closed.
The silicon carbide single crystal is produced according to a conventional PVT method, the seed crystal 7 is arranged above the inside of the crystal growth crucible 1, the raw material 8 is arranged below the inside of the crystal growth crucible 1, and the temperature in the crystal growth crucible 1 needs to be monitored so as to adjust the power of the heating device 5 in time.
EXAMPLE 5 application of PVT method to production of silicon carbide Single Crystal
The method comprises the following steps: silicon carbide single crystal (crystal form 4H) was produced according to the conventional PVT method using the heat radiation reflecting apparatus for producing silicon carbide single crystal and the method of using the same of example 1, wherein the thickness of the metal plating layer was set to different values.
The specific process for producing the silicon carbide single crystal by the PVT method comprises the following steps:
1) putting silicon carbide powder as a raw material 8 into a crucible 1; putting the seed crystal 7 into the inner top of the crucible 1, and sealing the crucible 1;
2) the crucible 1 is evacuated to an atmospheric pressure of 10-6Below mbar, introducing inert gas to 400mbar, repeating the process for 2-3 times, and finally pumping the gas pressure in the crucible 1 to 10-6mbar or more;
3) slowly raising the temperature in the crucible 1 to 1000 ℃, introducing inert gas into the crucible to raise the gas pressure to 700mbar, and keeping the gas pressure for 8 hours;
4) reducing the pressure in the crucible 1 to a single crystal growth pressure of 30mbar, and raising the temperature in the crucible 1 to 2200 ℃ for 150 hours under the condition of keeping the pressure in the crucible 1 unchanged;
6) after the growth of the single crystal is finished, the temperature and the pressure in the crucible 1 are reduced to room temperature and room pressure, the crucible 1 is opened, and the silicon carbide single crystal is taken out.
As a result: the results of the measurements of the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal are shown in table 1.
TABLE 1 results of experiments on the production of silicon carbide single crystal by PVT method using the apparatus of example 1
The results in Table 1 show that when the thickness of the coating Ta is less than 5 μm, the coating is not dense enough, the quality of the silicon carbide crystal cannot be improved obviously, and the energy consumption cannot be reduced obviously, and when the thickness of the coating Ta is 5-35 μm or more, the crystal quality (figure 5) can be improved obviously, and the energy consumption can be reduced obviously.
EXAMPLE 6 application of PVT method to production of silicon carbide Single Crystal
The method comprises the following steps: the process of example 5 was followed using the heat radiation reflecting apparatus for producing a silicon carbide single crystal of example 1.
As a result: the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal was examined as shown in table 2.
TABLE 2 results of experiments on the production of silicon carbide single crystal by PVT method using the apparatus of example 2
The results in tables 1 and 2 show that the coating Ta on the inner or outer wall of the quartz tube has no significant difference in the values of the parameters examined in the tables. I.e. the result of the coating Ta being provided in or outside the support is not significantly different.
EXAMPLE 7 application of PVT method to production of silicon carbide Single Crystal
The method comprises the following steps: the procedure of example 5 was followed except that: the vacuum isolation cover 3-1, namely the quartz tube, is internally provided with a tantalum carbide (TaC) coating.
As a result: the results of the measurements of the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal are shown in Table 3.
TABLE 3 Experimental results of the PVT method for producing silicon carbide single crystal
Comparative example 1 production of silicon carbide Single Crystal by PVT method without use of Heat radiation reflecting device
The method comprises the following steps: the procedure of example 5 was followed except that: the inner surface and the outer surface of the vacuum isolation cover 3-1 (namely, the quartz tube) made of quartz materials are not provided with the metal coating 6, and are provided with different types of circulating water cooling devices.
As a result: the results of the measurements of the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal are shown in Table 4.
TABLE 4 Crystal growth by circulating Water
The results of examples 5 and 6 and comparative example 1 show that, compared with cooling with circulating water, the use of the thermal radiation reflecting device in examples 5 and 6 significantly improves the crystal growth stability, effectively controls the crystal polytype defects, reduces the micropipe density, significantly improves the crystallization quality, and significantly reduces the consumption of electric energy during crystal growth and the cost.
Example 8 Effect of the Heat radiation reflecting device prepared by different methods on the production of silicon carbide Single Crystal by PVT Process
1. Different thermal radiation reflecting devices 1# -3# and D1# -D2# shown in table 5 were prepared according to the parameters shown in example 1 and table 5.
TABLE 5 preparation method of heat radiation reflection apparatus
2. According to the specific process for producing silicon carbide single crystals by the PVT method in example 5, the quality of the silicon carbide single crystals 1# -3# and D1#, D2# obtained by using the thermal radiation reflecting device 1# -3# and the comparative thermal radiation reflecting device D1# -D2# coated with a coating of 25 μm and the use of medium-frequency power during crystal growth were examined, as shown in Table 6.
TABLE 6 experimental results of PVT method for producing silicon carbide single crystal
The results in Table 6 show that when the roughness of the vacuum insulation cup satisfies the conditions, too large roughness of the surface of the plating layer results in poor crystal growth quality, for example, the microscopic polytype of the silicon carbide single crystal D1# becomes large, the crystal quality becomes poor, the amount of electricity used becomes large, and the like. However, in the case where the roughness of the surface of the plating layer is proper and the roughness of the surface of the vacuum insulation cover is not proper, that is, in the case of the lowermost sample close to the support, such as the silicon carbide single crystal D2#, the crystal quality becomes poor, but the amount of electricity used is also properly reduced because the connection of the plating layer to the support is not dense.
Those not described in detail in this specification are within the skill of the art. The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (13)
1. A heat radiation reflecting device for producing silicon carbide single crystals by a PVT method is characterized in that the heat radiation reflecting device can form a heat radiation reflecting mirror surface which can surround the periphery of a crystal growth crucible for producing the silicon carbide single crystals by the PVT method and can reflect heat emitted from the crucible back to the crucible;
the device for producing the silicon carbide single crystal by the PVT method does not comprise a cooling device or comprises the cooling device, but the cooling function of the cooling device is closed.
2. A thermal radiation reflecting device according to claim 1, comprising a specific material layer and a vacuum insulation cover, said vacuum insulation cover being capable of covering an outer periphery of said crucible, said specific material layer being provided on an inner surface of said vacuum insulation cover; or
The heat radiation reflecting device comprises a support and a specific material layer arranged on one side of the support;
the thermal radiation reflecting mirror surface is an outer surface of the specific material layer, and/or,
the heat radiation reflecting mirror surface is an interface between the support and the specific material layer, and the support is made of a transparent material.
3. A thermal radiation reflecting device according to claim 2, wherein an inner surface of said vacuum insulating cover is made of quartz; or
The support is quartz glass.
4. The thermal radiation reflection device according to claim 2, wherein the specific material is a metal, a silicon compound, a boride, a carbide, or a nitride;
the metal includes: tantalum, tungsten, molybdenum, iridium, niobium, germanium, hafnium, or alloys thereof;
the boride comprises: boron carbide, boron nitride, zirconium boride, lanthanum boride, titanium boride, tantalum boride, chromium boride, tungsten boride, molybdenum boride, vanadium boride, or niobium boride;
the carbide includes: chromium carbide, tantalum carbide, vanadium carbide, zirconium carbide, tungsten carbide, molybdenum carbide, titanium carbide, or niobium carbide;
the nitride includes: titanium nitride, tungsten nitride, molybdenum nitride, chromium nitride, niobium nitride, zirconium nitride, tantalum nitride, or vanadium nitride.
5. The thermal radiation reflection device as set forth in claim 4, wherein said specific material is a metal.
6. The thermal radiation reflection device defined in claim 4, wherein the metal is tantalum;
the carbide is tantalum carbide.
7. The thermal radiation reflection device according to claim 4, wherein said specific material is tantalum, and a thickness of said specific material layer is 3 μm or more;
and/or the roughness of the heat radiation reflecting mirror surface is less than 25 μm.
8. The thermal radiation reflection device as claimed in claim 7, wherein the thickness of said specific material layer is 4-100 μm; and/or
The roughness of the heat radiation reflecting mirror surface is less than 15 μm.
9. A thermal radiation reflection means according to claim 8, characterized in that said specific material layer has a thickness of 15-35 μm.
10. The method for producing a thermal radiation reflecting device according to any one of claims 2 to 9, characterized in that the method comprises coating an inner surface of the vacuum insulation cover or an inner surface or an outer surface of the support with a vacuum coating method to obtain the thermal radiation reflecting device in which the specific material layer and the thermal radiation reflecting mirror surface are formed on the inner surface of the vacuum insulation cover or on the inner surface or the outer surface of the support;
the vacuum coating method is sputtering coating, and the sputtering coating method comprises the following steps:
1) cleaning the vacuum isolation cover or the support as a substrate by using acetone and then deionized water, wherein the surface roughness of the substrate is not more than 10 microns;
2) background vacuum degree of shooting chamber is 1.0 x 10-4～9.9×10-4Pa or 1.0X 10-5～9.9×10-5Pa, introducing argon with the purity not lower than 99.99% into a coating chamber for 0.5-1 h before sputtering, and keeping the pressure at 0.1-1.5 Pa;
3) the metal with the purity not lower than 99.999% is used as a target material, the substrate is sputtered with the sputtering power of 40-60W, the sputtering gas is argon with the purity not lower than 99.99%, the gas pressure is 0.2-2.7 Pa, and the sputtering lasts for 2-3h, so that the heat radiation reflecting device with the metal as the specific material is obtained.
11. Use of the thermal radiation reflecting device according to any one of claims 1 to 9, or the thermal radiation reflecting device obtained by the method according to claim 10, in the production of a silicon carbide single crystal by the PVT method.
12. Use according to claim 11, for improving the quality of silicon carbide single crystals produced by the PVT method and/or for reducing the energy consumption for producing silicon carbide single crystals by the PVT method.
13. The use according to claim 12, wherein said improving the quality of the PVT process for producing single crystals of silicon carbide comprises: reducing crystal polytype, lattice distortion, micropipe number, and/or micropipe density in a silicon carbide single crystal.
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